Ambient pressure synthesis of zeolite films and their application as corrosion resistant coatings

a technology of zeolite and zeolite film, which is applied in the direction of liquid/solution decomposition chemical coating, chemical production of bulk materials, electric/magnetic/electromagnetic heating, etc., can solve the problems of chromate becoming more and more stringent, and affecting the synthesis process, so as to achieve the effect of drastically shortening the synthesis tim

Inactive Publication Date: 2010-05-13
RGT UNIV OF CALIFORNIA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0007]In accordance with another exemplary embodiment, a method for producing zeolite films or membranes at ambient pressure, comprises; preparing a synthesis mixture comprising an ionic liquid solvent and aluminum, and / or silicon, and / or phosphate sources; stirring the synthesis mixture, for example, at an elevated temperature; introducing a substrate; and heating the synthesis mixture and the substrate under conditions sufficient to form a continuous zeolite layer. In certain instances, the synthesis mixture can be stirred for approximately 4 hours (approximately 240 minutes) at 100 ° C. For example, the stirring requires at least 10 min at a temperature of less than 100° C. Exemplary temperature ranges include 80-100° C., 60-100° C., 40-80° C. and 60-80° C. In other instances, the synthesis mixture and the substrate can be heated to approximately 150° C. to form a continuous zeolite layer. In yet other instances, the synthesis mixture and the substrate can be heated for several hours to several days at a temperature from about 100 to 230° C. to form a continuous zeolite layer. Microwave heating can also be applied to this method of synthesizing zeolite films or membranes to accelerate the synthesis process. Surprisingly, the synthesis time can be drastically shortened by microwave heating. For example, in the presence of microwave heating, the synthesis time is from about 5 min to several hours, such as 2, 3, 4 or 5 hours.

Problems solved by technology

Metal corrosion is a widespread problem throughout the industrialized world, causing losses amounting to several percent of the gross domestic product of the typical industrialized country.
Unfortunately, chromate has become more and more stringently regulated since it is highly toxic and carcinogenic.

Method used

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  • Ambient pressure synthesis of zeolite films and their application as corrosion resistant coatings
  • Ambient pressure synthesis of zeolite films and their application as corrosion resistant coatings
  • Ambient pressure synthesis of zeolite films and their application as corrosion resistant coatings

Examples

Experimental program
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Effect test

example 1

AEL Coating Synthesis on Aluminum Alloys.

[0047]In accordance with an exemplary embodiment, both AIOPO-11 and SAPO-11 were synthesized on Al alloys. These alumino- and silicoalumino-phosphate zeolites have an AEL-type framework. A synthesis mixture with molar composition: 32[1-methyl-3-ethylimidazolium bromide ([emim]Br)]:1[Al(OC3H7)3]:3[H3PO4]:0.8[HF] was pre hours (approximately 240 minutes) at 100° C. For SAPO-11, tetraethyl orthosilicate (TEOS) was introduced to synthesis mixture with the molar ratio of 0.25Si:1AI. Metal substrates (i.e., AA 2024-T3 substrates) were pretreated by an Alconox detergent solution. The substrates were then fixed vertically inside the synthesis mixture in the Teflon vessel designed for MARS5 (CEM Co.) microwave reaction system. The unsealed vessel (with holes on the cover) was then quickly heated to 150° C. and held at the temperature for 2 hours (approximately 120 minutes) under microwave radiation. After the synthesis, the coated sample was thoroughl...

example 2

[0063]MEL PSZ nanocrystal suspension was synthesized in the following way: 9.15 g of tetrabutylammonium hydroxide (TBAOH, 40% aqueous solution, Sachem) and 4.67 g of double deionized (DDI) water were added into 10 g of tetraethylorthosilicate (TEOS, 98%, Aldrich). The mixture was stirred in a sealed plastic bottle for 24 hr at room temperature, and finally a clear homogeneous solution was formed with the molar composition of 0.3TBAOH:1SiO2:4EtOH:10H2O. The solution was then thermally treated at 80° C. for 2 days with constant stirring in an oil bath (noted as the first stage). Afterwards, a specific amount (varying from 10 wt % to 60 wt %) of solvent was evaporated out by house vacuum at room temperature with stirring. This solution was subsequently transferred to Teflon®-lined autoclaves and kept in a convection oven preheated at 114° C. for 24 hr (noted as the second stage). This synthesis approach is hereby referred to as an evaporation-assisted two-stage synthesis method. For co...

example 3

Silane-Zeolite Nanocrystal Coatings

[0067]In accordance with another exemplary embodiment, a 1,2-bis(triethoxysilyl)methane (BTSM) solution was prepared by adding silane to a DI water and ethanol mixture. The volume ratio of BTSM: DI water: Ethanol was approximately 1:1:20. Acetic acid was then added to adjust the pH of the solution in the range of approximately 4.5 to 5. The solution was then stirred at room temperature for aging at least 24 hours before a MEL suspension was added. MEL concentration in the solution was about 20 ppm (parts per million). Then the nanoparticle-silane mixture was spun on bare AI alloys or SAPO-11 coated AI Alloys at room temperature on a Laurell spin coater. Afterward, the sample was heated at 80° C. overnight and then 200° C. for 30 min (minutes).

Characterization

[0068]In accordance with another exemplary embodiment, the XRD patterns were obtained on Siemens D-500 diffractometer using Cu Kα radiation. SEM pictures were obtained on a Philips

[0069]XL30-FE...

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Abstract

A method for producing zeolite films or membranes at essentially ambient pressure, which includes preparing a synthesis mixture comprising an ionic liquid solvent and an aluminum and/or silicon and/or phosphate source and converting the synthesis mixture to form a continuous zeolite layer. In addition, a method of synthesizing zeolite nanocrystals, which includes preparing a synthesis mixture, the synthesis mixture having a silica or a silica and alumina source, and a template; and synthesizing the synthesis mixture to form zeolite nanocrystals.

Description

CROSS-REFERENCES TO RELATED APPLICATIONS[0001]This application claims priority to U.S. Provisional Patent Application No. 61 / 103,448 filed Oct. 7, 2008, which application is incorporated herein by reference in its entirety and for all purposes.STATEMENT AS TO RIGHTS TO INVENTIONS MADE UNDER FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT[0002]This invention was made with Government support under Grant No. DACA72-03-C-0007, awarded by the Department of Defense. The Government has certain rights to this invention.BACKGROUND OF THE INVENTION[0003]Metal corrosion is a widespread problem throughout the industrialized world, causing losses amounting to several percent of the gross domestic product of the typical industrialized country. Many types of metals are susceptible to corrosion, with aluminum alloys being prominent examples. The protection of metals against corrosion is generally achieved by applying a coating to the exposed surface of the metal to serve as a physical barrier between t...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): C01B39/02C01B39/54C01B39/04B05D1/36B05D3/10B05D1/18B05D3/06B05D3/12B05D3/02
CPCC01B39/36C23C18/1212C01B39/54C01B39/38Y02P20/54
Inventor YAN, YUSHANCAI, RUISUN, MINWEI
Owner RGT UNIV OF CALIFORNIA
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